Process and apparatus for producing emulsions



July 4, 1933. L. KIRSCHBRAUN PROCESS AND APPARATUS FOR PRODUbING EMULSIONS Original Filed March 14, 1929 j zz/klu aiq' Patented July 4, 1933 UNITED STATES LESTER KIRSCHBRAUN, OF LEONLA, NEW JERSEY, ASSIGNOR, BY MESNE ASSIGNMENTS,-

TO THE FLINTKOTE CORPORATION, OF BOSTON, MASSACHUSETTS, A CORPORATION OF MASSACHUSETTS PROCESS AND APPARATUS FOR PRODUCING EMULSION S Continuation of applicationflerlal No. 346,872, filed March 14, 1929. This application filed December 20,

1930. Serial No. 503,350,

This application is a continuation of my.

co-pending application Serial No. 346,872, filed March 14th, 1929.

Thepresent invention relates to improvements in the manufacture of emulsions, and has for its principal object to provide for an economical and highly efiicient continuous emulsifying and beating operation.

The improvements of the present invention are applicable particularly to aqueous emulsions or dispersions of normally solid or semi-solid bitumens, such as asphalt and the like, but in its broad aspects the invention is applicable to the production of aqueous dispersions of all substances of analogous nature normally immiscible with water.

Aqueous dispersions of materials of this I general group have been known for some time, and extensive quantities are being produced commercially at the present time in accordance with certain of the better known and more practical methods available in the art.

According to one method, a bulk supply of finished emulsion is maintained in an emulsifier. Emulsifying agent, water and waterimmiscible substance to be dispersed are introduced to the emulsifier, being agitated and intimately intermingled therein, undergoing emulsification and co-mingling with the bulk I supply. Regulated quantities of finished emulsion from the bulk supply are intermittently or continuously withdrawn. Under usual conditions of emulsification, the withdrawn product is generally of a paste-like consistency, that is, its viscosity is high.

.There are a number of commercial reasons for controlling the conditions of emulsification so as to maintain a relatively high viscosity-in the emulsifier, one of the important reasons being that it has been found that the maintenance of a high viscosity during emulsification results in a desirable fine degree of.

dispersion. Another obvious reason is that viscosity is in direct proportion to the amount of Water contained in the emulsion being withdrawn from the emulsifier, and the aim is to operate in such a way that the product being withdrawn from the emulsifier contains a minimum amount of water.

,fying zone with In application for commercial use, accordmg to one method, said-viscous emulsion can be readily diluted and thinned with water because of the fact that the water is in the external phase. Accordingto another meth- 0d, the viscous emulsion of paste-like consistency may be subjected to a controlled beating or Whipping action which it has been found materially increases the fluidity of the emulsion Without the use of that amount of water normally required for such decrease in'viscosity. This lattermethod is known as beating and is in extensive. commercialsecondary zone where a greater intensity of agitation, prevails, or through agitating zones of progressively increasing intensity.

According to' the process of the invention, eniulsification preferably continuously proceeds in the emulsifier in the presence of a bulk supply of end product. Regulated quantities of the relatively thick and highly viscous end product as withdrawn'f'rom the emulsifier are subjected to a controlled and progressive beating operation for progressively thinningthe same to a viscosity substantially below the normal emulsifying viscosity obtaining in the emulsifying zone, and,

as one of the features of the process, regu-. lated amounts of thinned emulsion are returned from the beating zone to the emulsiadvantages hereinafter more particularly brought out.

The apparatus of the present invention comprises in combination an emulsifier, a beater (zone of more intense agitating action passageways than prevails in the emulsifier) and valved communications between the emulsifier and beater, one for transferring end product from the emulsifier to the beater and the other for returning controlled amounts of thinned emulsion to the emulsifier.

By means of the process and apparatus herein described and claimed, I am enabled to produce a maximum quantity of finished emulsion of desired fluidity with a minimum water content by means of a relatively small compact apparatus, continuous daily pro- .duction in large volume being recognized commercially as the basis of economicaloperation.

Further utility of the invention as well as numerous other objects and advantages will be brought out in the following description.

In the drawing, Fig. 1 is a diagrammatic top plan view of the apparatus of the present invention. I

Fig. 2 is a vertical sectional view taken on line 22 of Fig. 1.

Referring more particularly to the drawing, the apparatus may comprise a pair of adjoining horizontally disposed elongated 1 and 2 of restricted cross section connected with. each other at both ends by communicating ducts 3 and 4 to permit cyclic circulation of material between the two passageways.

duit, designated as a whole at 6, which conduit according to the present invention takes the form of a U comprising parallel conduits 7 and 8 connected by the U bend 9. Preferably, parallel conduits 7 and 8 have free communication with each other through the medium of the open U bend 9.

lVithin the passageways 1 and 2 there are disposed fixed longitudinal shafts 10 mounted to rotate at a speed of to R. P. M.,

more or less, on which shafts are mounted The'emulsifying agent, which may com-- prise clay, bentonite, mineral pigments, colloidal oxides and hydroxides, silicates or other emulsifying media, may be introduced near one end of the passageway 1, as for example, through a feed pipe 13. As introduced to passageway 1, the emulsifying me-- dia may be in the form of either a thin aqueous suspension or a heavy aqueous paste, or

Passageway 2 is connect-' ed by means of channel 5 with a closed con-' may be introduced in dry condition, in which event water would be introduced through another feed pipe (not shown).

The emulsifying media is, forced along by the blades 11 in the passageway 1; the waterimmiscible material to be dispersed may be fed into the passageway 1 throu h either or ere por both of the feed pipes 14 or 14'. tions of the finished end product are beingrecycled to the passageway 1, as more-particularly described hereinafter, it is preferable to introduce the bitumen through the feed pipe '14 in order to permit the recycled material out recycling portions of the finished end product and/or where a prepared suspenslon of emulsifying agent is introduced through the feed line 13, the bitumen will preferably befed in through the feed ipe 14:. The

action of the helicoidal bla es 11 and the small propeller blades 12 in passageway 1 will serve to produce a mixing of the materials introduced, plus a forward, moving action through the trough land then through the connect-ion 3 into the adjacent parallel trough 2, the material being emulsified during its movement through these passageways. At the end of passageway 2, part of he emulsion may be discharged through the connecting conduit 4 to be recirculated through conduit 1, or part or all of the emulsion may be discharged through the connecting channel 5into the beating conduit 7, by obvious manipulation of the valves 15.

(londuit 7 is provided with a shaft 16 upon which are mounted a series of propellers or paddles 17 adapted to revolve preferably at a higher rate of speed than the shafts 10 so as to produce a more intense agitating effect than prevails in the passageways 1 and 2. For instance, thespeed of the shaft 16 may conveniently bearound 150 to 200 R. P. M., the propeller blades 17 forcing the emulsion along in conduit 7 in the direction of the arrows, discharging same into the conduit 9 connecting passageway 7 with passageway 8 where the material may be subjected to a still more intense agitating effect.

Conduit 8 is provided with a shaft 16 and propellers 17 similar to the shaft and propellers in conduit 7, but adapted to force the material along in a direction countercurrent to the direction of flow in conduit 7, as illusion iio

iis

iao

trated by the arrows. Preferably, the shaft 16 in conduit 8 is geared to rotate at a much whereby to effect a more intense agitating action.

Any modifying agent, such, fdr instance, as chromate, material for pH adjustment, or any other type of modifying agent may be added to he emulsion, as for example, prior to the final stage of agitation, through conduit 18. The finished material may be withdrawn from conduit 8 through outlet 19.

As a feature of the present invention, regulated amounts of'the finely thinned material may be diverted from conduit 8 and out- .let 19 and returned through connecting channl 20 to the first emulsifying trough 1, where it can be brought to desired consistency by mixture with the emulsifying agent introduced at 13, or with emulsion recirculated from trough 2 through communicating duct 4, or both. A valve 21 is interposed in the draw-off pipe 19 for controlling the withdrawal of finished emulsion. from the conduit 8'. By regulating the height of the overflow through draw-off l9 finished material can be drawn off at the desired rate.

The conduits 1, 2, 7 and 8 are preferably jacketed, as shown in thedrawing, to provide for the introducing of a temperature regulating medium. In conduits 7 and 8 it is frequently found necessary to cool the material because considerable heat is developed by friction which must be dissipated more rapidly than is possible through the action of the surrounding atmosphere in order to secure the best results, and therefore, cooli ng liquid is applied to the jackets 7' an 8 through valved inlet 7" and withdrawn through valved outlet Q'C,

To produce an emulsion of minimum water content, it is important to cool the material in the zones of higher agitation as much and as quickly as possible, for the more quickly gthe temperature is reduced during the thinning stage, the lower is thewater content for a given consistency. In general, during the stage'in which the particlesize is being reduced, the temperature shouldbe maintained close to the melting point of the bitumen be-- ing emulsified, but when the desired particle size has been obtained, the temperature should be dropped as quickly as possible and to as low adegree as the cooling medium permits, the eflluent material being preferably approximately 70 F. v r

There are many advantages in returning product from conduit 8 to the initial emlilsifying trough 1, for instance, this afl'ordsa means ofmore accurately controlling the operation and having it run more smoothly.

Also, by thus returning some of the finished material, the emulsion can be made with a water content much lower than is otherwise pqssible. The relative quantities of final product returned from conduitv 8 to condult 1 willidepend entirely upon the material beregulated amounts of the cooled, thinned final scribed is designed to produce emulsion continuously and subject the emulsion, after the particles have been brought into an initial state of subdivision, to a beating action for reducing the viscosity of the emulsion as formed, or for producing further subdivision of the particles in the zones of more intense agitation, and, as a. feature of the invention, theprocess and apparatus is designed to return to the emulsifying zone regulated quantities of the cooled, thinned finished product, wherebyemulsions of minimum water content for a given consistency may be economically produced. Thus, for example, wherebentonite' is used as an emusifying agent without carrying the material through agitating zohes. of successively increasing inmg a spreading consistency, is generally about.45%, but by meansof the aforesaid feature of my invention, an emulsion of the same degree of fluidity and corresponding particle size may be produced with a water no content of only 36 to 38%. Furthermore, by cooling quickly the material passing through the zones of higher intensity of agitation, the water content may be still further reduced to about 30 to 32%, especially where portions of the finished material are recycled as described, to the zone of initial emulsification.

I claim as my-invention;

1. A process which comprises mixing and agitating water-immiscible material with no vwater to produce a dispersion in which the water to produ ce'a dispersion in which the water-immiscible material constitutes the i-nternal phase and the water the external phase,su bjecting said dispersion to a more intense agitating action, thereafter combin- I ing regulated portions of finished emulsion with the materials being mixed and agitated in the initial dispersing stage and introducing to the initial dispersing stage regulated produce a dispersion in which water=1m-' *phase,

amounts'o'f fresh'materials to be mixed' and agitated to produce dispersion.

- 3. An apparatus comprising an emulsifier wherein materials are mixed and agitated to miscible material constitutes the internal phase and water constitutes the external a beater wherein said dispersionis subjected to a more a valved communication between the emulsiamounts of thinned dispersion 99 increase the fluidity thereof,

Mwherein materials are mixed and \fier and'said heater for dischargingemulsion,

emulsifier for returningregulated amounts means for charging of thinned dispersion to said emulsifier, fresh materials to be mixed and agitated to said emulsifier, and a valved outlet from said beater for withdrawing the thinned final product.

5. A process which comprises mixing and agitating water-immiscible material with water to produce a dispersion of paste-like consistency in which the water-immiscible material constitutes the internal phase and the water the external phase, subjecting said dispersion of paste-like consistency to a beating or whipping action to render same more fluid, and thereafter returning regu-' lated portions'of said thinned dispersion to j progressively decrease to below the normal emulsifying the zone where the initial dispersion of paste-like consistency is produced. a

6. A process which comprises commin-' gling heat liquefied bitumen with a mixture of water and emulsifyingagent, agitating the, commingled mass to etfect emulsification of the bitumen, subjecting'the emulsion thus under conditions to the viscosity thereof viscosity of the bitumen and lowering the temperature produced to agitation of the mass rapidly during said last named agitation. p

7. A continuous process WhlCh comprises intense'agitating action,

agitated to' commingling heat liquefiedbitumen with a mixture of water and emulsifying agent, ag tating the commingled mass to efiect emuls1- fication, of the-bitumen while-maintaining the temperature of the mass substantially at the melting point of the bitumen, subjecting the emulsion thus produced to a itation under conditions to progressively ecrease the viscosity thereof below. the normal emulsifying viscosity of the bitumen and lowering the temperature of the mass rapidly during said last named agitation to a temperature substantially below the melting point of the bitumen.

- 8. A process which comprises commmghng heat liquefied bitumen with a mixture of water and emulsifying agent, agitating the commingled mass to effect emulsification of the bitumen, passing the emulsion thus produced through agltating zones of progressively increasing intensity to cause a progressive decrease in viscos ty of the emulsion, while simultaneously rapidly decreasing the temperature of the emulsion to substantially below the melting point of thebitumen and withdrawing the emulsion 'of reduced viscosity from the last named z'one.

9. A continuous process which comprises commiligling and agitating bitumen with a mixture of water and emulsifying agent to form an emulsion, passing the emulsion thus formed through a zone, separate and distinct from the emulsifying zone, where it is subjected to intense agitation for reduction in viscdsity thereof to below the normal emulsifying viscosity of the bitu-. men, rapidly and substantially cooling the emulsion during said last named agitation and withdrawing the finished product from said last named zone. 1

heat liquefied '10. A continuous process which comprises commingling heat liquefied bitumen with a,

to form an emulsion, passing, 

